反应详情

温度

110 °C

Ethyl 2′-chloro-4′-methoxybiphenyl-2-carboxylate (67.7 g) was dissolved in ethanol (100 ml), 4N aqueous sodium hydroxide (100 ml) was added, and the mixture was stirred at an oil bath temperature of 110° C. for 4.5 hr. The reaction mixture was cooled to room temperature, water (200 ml) and toluene (100 ml) were added, and the mixture was stirred overnight. To the reaction mixture was added activated carbon (3.6 g), and the mixture was further stirred for 1 hr. The insoluble material was filtered off through celite, and the insoluble material was washed with toluene (30 ml) and water (300 ml). The obtained filtrates were combined to allow for layer separation. The obtained aqueous layer was washed with toluene (100 ml), the aqueous layer was acidified with concentrated hydrochloric acid (40 ml), and stirred at room temperature for 1 hr. The precipitated solid was collected by filtration. The obtained solid was air-dried for 3 hr, and dried under reduced pressure at 60° C. overnight to give the title compound (50.2 g).

1. temperatureThe reaction mixture was cooled to room temperature
2. stirringthe mixture was stirred overnight
3. additionTo the reaction mixture was added activated carbon (3.6 g)
4. stirringthe mixture was further stirred for 1 hr
5. filtrationThe insoluble material was filtered off through celite
6. washthe insoluble material was washed with toluene (30 ml) and water (300 ml)
7. customto allow for layer separation
8. washThe obtained aqueous layer was washed with toluene (100 ml)
9. stirringstirred at room temperature for 1 hr
10. filtrationThe precipitated solid was collected by filtration
11. customThe obtained solid was air-dried for 3 hr
12. customdried under reduced pressure at 60° C. overnight